CN102794281A - Method for washing graphite piece in thermal field of Czochralski single-crystal furnace - Google Patents
Method for washing graphite piece in thermal field of Czochralski single-crystal furnace Download PDFInfo
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- CN102794281A CN102794281A CN2012102325390A CN201210232539A CN102794281A CN 102794281 A CN102794281 A CN 102794281A CN 2012102325390 A CN2012102325390 A CN 2012102325390A CN 201210232539 A CN201210232539 A CN 201210232539A CN 102794281 A CN102794281 A CN 102794281A
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Abstract
The invention discloses a method for washing graphite piece in a thermal field of a Czochralski single-crystal furnace. The method is implemented by the following specific operation steps of: mounting the graphite piece; starting a furnace body cooling water circulation system and a power supply cooling water circulation system of a high-temperature induction furnace respectively; vacuumizing; heating including a preheating process and a heating process, carrying out the heating process according to a temperature rise manner of 100 DEG C per hour during temperature rise before realizing 1,000 DEG C, carrying out the heating process according to a temperature rise manner of 50 DEG C per hour during 1,000-2,000 DEG C temperature rise, and carrying out the heating process according to a temperature rise manner of 30 DEG C per hour during 2,000-2,400 DEG C temperature rise; uniformly cooling the interior of the high-temperature induction furnace from 2,4000 DEG C to 80-100 DEG C as the temperature of furnace discharge; and discharge the graphite piece. According to the method for washing the graphite piece in the thermal field of the Czochralski single-crystal growth furnace, disclosed by the invention, SiC reacts at high temperature so that the service life of the graphite piece is prolonged to be 15-30 furnaces, and the method disclosed by the invention is suitable for washing each graphite piece in the single-crystal furnace.
Description
Technical field
The invention belongs to the monocrystalline silicon production technical field, relate to the cleaning method of the graphite piece in a kind of Czochralski method mono-crystal furnace thermal field.
Background technology
The growing method of monocrystalline silicon is representative with Czochralski method (vertical pulling method) mainly.Form graphite crucible that Czochralski method mono-crystal furnace thermal field critical piece has the single-lobe block to be combined into, insulator, heater, heat shielding, heat-preservation cylinder, crucible holder, insulation cover etc.
Graphite piece in the following text is meant graphite crucible, insulator, heater, heat shielding, crucible holder.
In czochralski process, temperature is higher than 1400 ℃ in the single crystal growing furnace, and silica crucible is at high temperature softening, and reacting with polycrystalline silicon raw material generates SiO gas thus.SiO gas continues and the graphite piece reaction, generates carbon monoxide, carborundum etc., thereby causes the corrosion to graphite piece, and its reaction equation is following:
SiO
2+Si=2SiO，SiO+2C=SiC+CO，SiO
2+C=SiO+CO。
In the crystal pulling process, the mixture of high temperature, low pressure and silicon vapor can cause the generation carborundum that reacts between silicon and the graphite piece, and it is dark more that long more carborundum of reaction time penetrates graphite piece.
Carborundum has different thermal coefficient of expansions with graphite, and when carborundum reached certain depth, graphite piece will be broken, and had reduced the service life of graphite piece; Carborundum also is prone to and the silica crucible reaction, makes the silica crucible attenuation, makes silica crucible cause leakage silicon easily, and it is high to increase production cost.
Summary of the invention
The cleaning method that the purpose of this invention is to provide the graphite piece in a kind of Czochralski method mono-crystal furnace thermal field has solved and can't remove SiC corrosion layer on the graphite piece in the prior art, causes graphite piece short service life, the problem that production cost increases.
The technical scheme that the present invention adopted is, the cleaning method of the graphite piece in a kind of Czochralski method mono-crystal furnace thermal field is implemented according to following operating procedure:
The graphite piece that has the SiC corrosion layer after pulling of crystals used is packed in the high temperature induction furnace, then sealed lid;
The control parameter is omnidistance body of heater cooling circulating water: 20-25M
3/ h, omnidistance power supply cooling circulating water: 76-82M
3/ h;
Step 3, vacuumize
With being vacuumized by normal pressure in the high temperature induction furnace, furnace pressure begins to heat high temperature induction furnace during to 20-100Pa;
Step 4, heating
4.1) preheating: in the high temperature induction furnace during less than 100Pa, preheating 10-15min under 100 ± 10KW power;
4.2) heating up: high temperature induction furnace heats 20min under 200 ± 10KW power, continue heating 20min under 400 ± 10KW power, and the power with 600-650KW heats at last;
4.3) constant temperature 1h when temperature in the high temperature induction furnace reaches 1000 ℃, the heating power of high temperature induction furnace is 200 ± 10KW during constant temperature;
4.4) after constant temperature accomplished, the adjusting heating power was 300-400KW, with being warmed up to 1500 ℃ in the high temperature induction furnace;
4.5) constant temperature 1h when the interior temperature of high temperature induction furnace reaches 1500 ℃, heating power is 230-240KW during constant temperature;
4.6) to regulate heating power again be 600 ± 10KW, make to be warmed up to 2000 ℃ in the high temperature induction furnace;
4.7) constant temperature 1h when the interior temperature of high temperature induction furnace reaches 2000 ℃, heating power is 300 ± 10KW during constant temperature;
4.8) to regulate high temperature induction furnace power be 600-650KW, with being warmed up to 2400 ℃ in the high temperature induction furnace;
4.9) when temperature reaches 2400 ℃ in the high temperature induction furnace, constant temperature 2-6h, heating power is 430-450KW during constant temperature, vacustat is constant and stop heating during less than 100Pa;
Step 5, cooling
Guarantee the logical cooling water of high temperature induction furnace body of heater during cooling, lead to nitrogen simultaneously in the high temperature induction furnace as protective gas, the cooling of lowering the temperature; Use 130-140h, tapping temperature with temperature in the high temperature induction furnace from 2400 ℃ of uniform decrease in temperature to 80-100 ℃;
Step 6, graphite piece are come out of the stove.
The invention has the beneficial effects as follows: 1) through SiC is at high temperature reacted, reduce the corrosion of SiC, prolong the 15-30 stove in service life of graphite piece graphite piece and silica crucible.2) applied widely, promptly be applicable to the cleaning of each graphite piece in the single crystal growing furnace.
Description of drawings
Fig. 1 is the graphite piece schematic cross-section of existing non-defective unit;
Fig. 2 is that graphite piece is used the schematic cross-section after a period of time produces corrosion.
Among the figure, 1. graphite linings, 2. silicon carbide layer.
The specific embodiment
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is elaborated.
With reference to Fig. 1, the main part of the graphite piece of non-defective unit is graphite linings 1 entirely.
With reference to Fig. 2, after graphite piece use a period of time generation corrosion, the inner surface of its graphite linings 1 is converted into silicon carbide layer 2 (claiming corrosion layer again).
The present invention is the cleaning method of the graphite piece in a kind of Czochralski method mono-crystal furnace thermal field; Its principle is to utilize chemical method to remove the silicon carbide layer that produces in the monocrystalline silicon production process 2; Make silicon carbide layer 2 that reduction reaction at high temperature take place, convert carbon and silicon vapor into, regression equation is: SiC (s)=2Si (g)+C (s); Thereby reach the purpose that graphite piece is cleaned, prolong graphite piece service life with this.
The cleaning method of the graphite piece in the Czochralski method mono-crystal furnace thermal field of the present invention, implement according to following concrete operating procedure:
The graphite piece that has the SiC corrosion layer after pulling of crystals used is packed in the high temperature induction furnace, and sealed lid will be put when packing into rationally then, in order to avoid damage graphite piece;
The control parameter is omnidistance body of heater cooling circulating water: 20-25M
3/ h, omnidistance power supply cooling circulating water: 76-82M
3/ h;
Step 3, vacuumize
With being extracted into vacuum by normal pressure in the high temperature induction furnace, furnace pressure begins to heat high temperature induction furnace during to 20-100Pa; Will make graphite piece oxidized if the air pressure in the high temperature induction furnace surpasses 100Pa, therefore, the pressure in the high temperature induction furnace is more little good more;
Step 4, heating
4.1) preheating: in the high temperature induction furnace during less than 100Pa, preheating 10-15min under 100 ± 10KW power;
4.2) heating up: high temperature induction furnace heats 20min under 200 ± 10KW power, continue heating 20min under 400 ± 10KW power, and the power with 600-650KW heats at last; Before 1000 ℃ in the temperature-rise period, carry out according to 100 ℃ intensification amplitude per hour,
The power of high temperature induction furnace controlled well progressively heats, and 10 hours altogether, if heating is too fast, can make graphite piece expand with heat and contract with cold and break, and this progressively mode of heating also can help to protect the body of heater of high temperature induction furnace;
4.3) constant temperature 1h when temperature in the high temperature induction furnace reaches 1000 ℃, the heating power of high temperature induction furnace is 200 ± 10KW during constant temperature; Temperature constant state is in order to protect single crystal growing furnace, if it is too fast to heat up, can produces and expand with heat and contract with cold, and long-term use meeting causes damage to single crystal growing furnace, shortens the service life of single crystal growing furnace;
4.4) after constant temperature accomplished, the adjusting heating power was 300-400KW, with being warmed up to 1500 ℃ in the high temperature induction furnace;
4.5) constant temperature 1h when the interior temperature of high temperature induction furnace reaches 1500 ℃, heating power is 230-240KW during constant temperature;
4.6) to regulate heating power again be 600 ± 10KW, make to be warmed up to 2000 ℃ in the high temperature induction furnace; In 1000-2000 ℃ of temperature-rise period, carry out according to 50 ℃ intensification amplitude per hour;
4.7) constant temperature 1h when the interior temperature of high temperature induction furnace reaches 2000 ℃, heating power is 300 ± 10KW during constant temperature;
4.8) to regulate high temperature induction furnace power be 600-650KW, with being warmed up to 2400 ℃ in the high temperature induction furnace; In 2000-2400 ℃ of temperature-rise period, carry out according to 30 ℃ intensification amplitude per hour;
4.9) when temperature reaches 2400 ℃ in the high temperature induction furnace, constant temperature 2-6h, heating power is 430-450KW during constant temperature, vacustat is constant and stop heating during less than 100Pa.
Step 5, cooling
Guarantee the logical cooling water of high temperature induction furnace body of heater during cooling, lead to nitrogen simultaneously in the high temperature induction furnace as protective gas, the cooling of lowering the temperature; Use 130-140h, tapping temperature with temperature in the high temperature induction furnace from 2400 ℃ of uniform decrease in temperature to 80-100 ℃.
Step 6, graphite piece are come out of the stove.
The every use of following contrast experiment's graphite piece 5-10 stove just adopts said method to clean once, compares with unwashed graphite piece, and contrast and experiment is shown in following table 1, table 2:
Table 1: contrast in service life before and after graphite crucible cleans
Above graphite crucible, the graphite crucible that did not clean have two stoves to occur leaking the silicon phenomenon, and the silicon phenomenon does not appear leaking in the graphite crucible that cleaned.
Table 2: contrast in service life before and after heater cleans
In sum; The cleaning method of the graphite piece in the Czochralski method mono-crystal furnace thermal field of the present invention; The graphite piece that produces certain thickness silicon carbide layer because of corrosion in the monocrystalline silicon production process 2400 ℃ of temperature, is carried out chemical reduction reaction under the condition of reacting furnace pressure≤100Pa, realize the graphite piece cleaning.Step is simple, and rehabilitation cost is low, and cleaning performance is good, is applicable to the cleaning of each graphite piece in the single crystal growing furnace fully.
Claims (2)
1. the cleaning method of the graphite piece in the Czochralski method mono-crystal furnace thermal field is characterized in that, implements according to following steps:
Step 1, installation graphite piece
The graphite piece that has the SiC corrosion layer after pulling of crystals used is packed in the high temperature induction furnace, then sealed lid;
Step 2, open the body of heater cooling water recirculation system and the power supply cooling water recirculation system of high temperature induction furnace respectively
The control parameter is omnidistance body of heater cooling circulating water: 20-25M
3/ h, omnidistance power supply cooling circulating water: 76-82M
3/ h;
Step 3, vacuumize
With being vacuumized by normal pressure in the high temperature induction furnace, furnace pressure begins to heat high temperature induction furnace during to 20-100Pa;
Step 4, heating
4.1) preheating: in the high temperature induction furnace during less than 100Pa, preheating 10-15min under 100KW power;
4.2) heating up: high temperature induction furnace heats 20min under 200KW power, continue heating 20min under 400KW power, and the power with 600-650KW heats at last;
4.3) constant temperature 1h when temperature in the high temperature induction furnace reaches 1000 ℃, the heating power of high temperature induction furnace is 200KW during constant temperature;
4.4) after constant temperature accomplished, the adjusting heating power was 300-400KW, with being warmed up to 1500 ℃ in the high temperature induction furnace;
4.5) constant temperature 1h when the interior temperature of high temperature induction furnace reaches 1500 ℃, heating power is 230-240KW during constant temperature;
4.6) to regulate heating power again be 600KW, make to be warmed up to 2000 ℃ in the high temperature induction furnace;
4.7) constant temperature 1h when the interior temperature of high temperature induction furnace reaches 2000 ℃, heating power is 300KW during constant temperature;
4.8) to regulate high temperature induction furnace power be 600-650KW, with being warmed up to 2400 ℃ in the high temperature induction furnace;
4.9) when temperature reaches 2400 ℃ in the high temperature induction furnace, constant temperature 2-6h, heating power is 430-450KW during constant temperature, vacustat is constant and stop heating during less than 100Pa;
Step 5, cooling
Guarantee the logical cooling water of high temperature induction furnace body of heater during cooling, lead to nitrogen simultaneously in the high temperature induction furnace as protective gas, the cooling of lowering the temperature; Use 130-140h, tapping temperature with temperature in the high temperature induction furnace from 2400 ℃ of uniform decrease in temperature to 80-100 ℃;
Step 6, graphite piece are come out of the stove.
2. the cleaning method of the graphite piece in the Czochralski method mono-crystal furnace thermal field according to claim 1 is characterized in that: in the described step 2, before 1000 ℃ in the temperature-rise period, carry out according to 100 ℃ intensification amplitude per hour; In 1000-2000 ℃ of temperature-rise period, carry out according to 50 ℃ intensification amplitude per hour; In 2000-2400 ℃ of temperature-rise period, carry out according to 30 ℃ intensification amplitude per hour.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109338458A (en) * | 2018-12-21 | 2019-02-15 | 保定顺天新材料股份有限公司 | Monocrystaline silicon stove repairs the process of corrosion layer with charcoal charcoal guide shell |
| US20220267923A1 (en) * | 2021-02-25 | 2022-08-25 | Globalwafers Co., Ltd. | Purification apparatus and method of purifying hot zone parts |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1367275A (en) * | 2001-01-20 | 2002-09-04 | 上海德波赛康科研有限公司 | Preparation method of block silicone carbide monocrystal growth |
| CN1865528A (en) * | 2006-04-21 | 2006-11-22 | 天津市环欧半导体材料技术有限公司 | Large-diameter zone-melting silicon single crystal growth method |
| CN101623695A (en) * | 2009-08-13 | 2010-01-13 | 合肥景坤新能源有限公司 | Method for cleaning graphitic silicon materials |
| CN101798704A (en) * | 2009-12-31 | 2010-08-11 | 峨嵋半导体材料研究所 | Process for growing phi 8'' solar-grade Czochralski silicon by using 18-inch thermal field |
| CN102391015A (en) * | 2011-07-27 | 2012-03-28 | 西安交通大学 | SiC ceramic surface treatment method and application thereof |
-
2012
- 2012-07-06 CN CN201210232539.0A patent/CN102794281B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1367275A (en) * | 2001-01-20 | 2002-09-04 | 上海德波赛康科研有限公司 | Preparation method of block silicone carbide monocrystal growth |
| CN1865528A (en) * | 2006-04-21 | 2006-11-22 | 天津市环欧半导体材料技术有限公司 | Large-diameter zone-melting silicon single crystal growth method |
| CN101623695A (en) * | 2009-08-13 | 2010-01-13 | 合肥景坤新能源有限公司 | Method for cleaning graphitic silicon materials |
| CN101798704A (en) * | 2009-12-31 | 2010-08-11 | 峨嵋半导体材料研究所 | Process for growing phi 8'' solar-grade Czochralski silicon by using 18-inch thermal field |
| CN102391015A (en) * | 2011-07-27 | 2012-03-28 | 西安交通大学 | SiC ceramic surface treatment method and application thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109338458A (en) * | 2018-12-21 | 2019-02-15 | 保定顺天新材料股份有限公司 | Monocrystaline silicon stove repairs the process of corrosion layer with charcoal charcoal guide shell |
| CN109338458B (en) * | 2018-12-21 | 2020-10-30 | 保定顺天新材料股份有限公司 | Process method for repairing corrosion layer by using carbon-carbon guide cylinder for monocrystalline silicon furnace |
| US20220267923A1 (en) * | 2021-02-25 | 2022-08-25 | Globalwafers Co., Ltd. | Purification apparatus and method of purifying hot zone parts |
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Address after: The new town in the county the Ningxia Hui Autonomous Region city centre 755100 unity Road Co-patentee after: Yinchuan LONGi Silicon Material Co.,Ltd. Patentee after: Ningxia LONGi Silicon Material Co.,Ltd. Co-patentee after: Longji green energy Polytron Technologies Inc Co-patentee after: Wuxi LONGi Silicon Materials Corp. Address before: The new town in the county the Ningxia Hui Autonomous Region city centre 755100 unity Road Co-patentee before: Yinchuan LONGi Silicon Material Co.,Ltd. Patentee before: Ningxia LONGi Silicon Material Co.,Ltd. Co-patentee before: Xi'an Longji-Silicon Co., LTD. Co-patentee before: Wuxi LONGi Silicon Materials Corp. |
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Granted publication date: 20140618 Termination date: 20200706 |
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